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K00326 - 20181121132815 - Lab Manual SKU1023
K00326 - 20181121132815 - Lab Manual SKU1023
K00326 - 20181121132815 - Lab Manual SKU1023
LABORATORY MANUAL
SKU 1023 BASIC CHEMISTRY II
STUDENT’S NAME
MATRIC NO.
LECTURER’S/TUTOR’S NAME
DAY/TIME
LABORATORY
SKU 1023
BASIC CHEMISTRY II
NO EXPERIMENT
2 Titration of acid-base
5 Galvanic cell
Instruction for writing the lab report
OBJECTIVE
Upon completion the experiment, students should be able to:
1. Prepare and standardise the concentration of NaOH and HCl solution.
INTRODUCTION
During a titration, the volume of one reagent, the analyte (solution in Erlenmeyer flask) is
predetermined while the other reagent, the titrant (in burette) slowly introduced to the analyte
solution. The completion of this reaction can be determined via observation through the use of an
indicator. The amount of reagents is determined by knowing exactly volume of known molarity that
required to completely react with the analyte. Knowledge on the ratio of reaction between acid and
base allows determination of the other solution's Molarity.
Two basic methods are used to establish the concentration of such solution. There are:
1. The direct method in which a carefully weighed quantity of a primary standard compound is
dissolved in a soluble solvent and diluted to a known volume in a volumetric flask.
2. Standardization of the solution for titration analysis where the titrant (or titration reagent e.g.
NaOH) need to be standardized before using for determination of the concentration of other
solution. This process can be performed via titrating the titrant against.
a. A weighed quantity of primary standard (in solution form).
b. A weight quantity of secondary standard (in solution form).
c. A measured volume of another solution.
A titrant that is standardized against a secondary standard or against another solution is sometimes
referred to as a secondary standard solution. The concentration of a secondary solution is subject
to a larger uncertainty than that to a primary standard solution.
APPARATUS
Analytical balance, weighing bottle, Erlenmeyer flask, beaker 100 mL, volumetric flask 250 mL and
500 m, pipette 20 mL and 25 mL, burette 50 mL
REAGENTS
Sodium hydroxide, hydrochloric acid (0.3 M), oxalate acid dehydrate, distilled water, phenolphthalein
indicator
PROCEDURE
1. Refill and zero the NaOH burette. Read the NaOH level to within ± 0.02 mL and record this
value in the initial base reading on the data sheet.
2. Obtain a clean, but not necessarily dry, 250 mL Erlenmeyer flask , and using the burette
labeled "HCl" (located at the back of the room), transfer approximately 25.00 mL of the HCl
acid solution into the flask. Read and record the initial and final acid burette readings to ±
0.02 mL. It is not necessary to deliver exactly 25.00 mL of HCl into the flask. What is
important, is that the volume of HCl delivered into the flask is known to two decimal places.
3. Add 3 to 4 drops of phenolphthalein indicator to the HCl solution in the Erlenmeyer flask.
4. Place the flask containing the acid solution and indicator under the burette and add NaOH
from the burette to the flask with swirling until a phenolphthalein endpoint is reached. There
should be a one-drop difference between when the solution is colorless and when it is pink.
If too much base is added (that is, if you "over-shoot" the endpoint), discard the solution
and repeat the titration.
5. When the proper end point is reached, read and record the final NaOH volume to within ±
0.02 mL.
6. Discard the contents of the Erlenmeyer flask into the waste container located under the
hood. Repeat the titration procedure three time by following steps 1 - 5.
7. Calculate an average acid molarity using the two closest values.
8. Before returning the burette to the lab bench, please rinse it out with a couple of water
rinses.
Notes
1. Repeat the titration process at least three times to calculate the concentration. The
relative deviation between the results must be below than 3. Do the calculation of
deviation for every set reading.
2. Show your result to your demonstrator and get the real value. Calculate the error
percentage of your result.
DATA AND CALCULATIONS
DISCUSSION
1. Give the true formula of oxalate acid dehydrate and its molar mass.
2. List sources of possible error in the experiment.
EXPERIMENT 2
TITRATION OF ACID AND BASE
OBJECTIVE
Upon completion the experiment, students should be able to:
1. Determine the concentration of acid solution.
INTRODUCTION
Acid base titration involves a neutralization reaction in which an acid is reacted with an equivalent
amount of base. Neutralization occurs when acid and base exists in comparable stoichiometry, for
instance the amount of hydrochloric acid (mole) is equivalent with the amount of sodium hydroxide
(mole). The end point of titration can be determined using indicator.
Since 1 mole H+ uses up completely 1 mole of OH-, it follows that the complete neutralization requires
that the number of moles of acid (na) be equal to the number of moles of base (nb):
na = nb
This relationship can be combined with the definition of molarity:
na = Ma x Va and nb = Mb x Vb
Ma = Molarity of the acid Mb = Molarity of the base
Va = Volume of acid Vb = Volume of base
It follows that:
Ma x Va = Mb x Vb
The last relationship applies whenever the acid and base react in a 1:1 mole ratio.
However, the stoichiometry becomes more complex when the acid and base release unequal
number of H3O+ and OH- ions. The neutralization of sulfuric acid with sodium hydroxide is
expressed by the balanced chemical equation:
H2SO4 (aq) + 2NaOH (aq) Na2SO4 (aq) + 2H2O (l)
The 1:2 ratio of the acid to the base in the balanced equation indicates that twice as many moles of
base are needed than of acid:
2na = nb
2(Ma x Va) = Mb x Vb
In this experiment, you are going to determine the concentration of acid solution using NaOH (from
previous experiment).
APPARATUS
Analytical balance, weighing bottle, Erlenmeyer flask, volumetric flask 250 mL, pipette 20 mL and 25
mL, burette 50 mL
REAGENTS
Acid solution (X (HX) and Y(H2X)), NaOH standardize solution from previous experiment (~ 0.2 M),
distilled water, phenolphthalein indicator
PROCEDURE
1. Pipette 25 mL of X acid solution into 250 mL volumetric flask. Dilute with distilled water until
reach the mark. Invert the flask.
2. Fill up the burette with NaOH solution standardized in previous experiment.
3. Pipette 25 mL of X solution into Erlenmeyer flask. Add 3 to 4 drops of phenolphthalein
indicator to the X solution in the Erlenmeyer flask.
4. Note down the volume of NaOH required to completely react with acid.
5. Repeat the titration at least 3 times (be sure the volume of acid solution is consistent).
6. Calculate the concentration of X using NaOH solution.
7. Calculate the stock solution of X before dilution.
8. Repeat steps 1-7 for the titration of Y acid solution using NaOH.
DATA
Acid X
Titration 1 Titration 2 Titration 3
Initial NaOH buret reading (mL)
Final NaOH buret reading (mL)
Volume NaOH (mL)
Average NaOH (mL)
Acid Y
Titration 1 Titration 2 Titration 3
Initial NaOH buret reading (mL)
Final NaOH buret reading (mL)
Volume NaOH (mL)
Average NaOH (mL)
CALCULATIONS
DISCUSSION
QUESTIONS
OBJECTIVE
Upon completion the experiment, students should be able to:
1. Determine the solubility product constant Ksp for lead(II) iodide.
INTRODUCTION
Most ionic compounds are soluble in aqueous solution. However, some salts are insoluble or
sparingly soluble. In such cases, the extent to which the salt dissolves can be expressed using an
equilibrium expression.
In a saturated solution of an ionic solid, an equilibrium exists between the ions in the solution and
any undissolved solid. For example, the equilibrium equation for a saturated solution of lead chloride
(a sparingly soluble salt) in contact with the solid phase is:
PbCl2 (s) Pb2+ (aq) + 2Cl- (aq)
Even though no observable change is taking place in the system represent by this equation, a
dynamic equilibrium exists. The solid dissociates into ions at the same rate that the ions recombine
to form the solid. As long as the temperature remains constant, the concentrations of all components
of the system remain constant.
The concentration of ions in a saturated solution of a sparingly soluble salt (e.g. PbCl 2) will usually
be very small. It has been determined that for such solutions, the product of the molar concentrations
(moles/liters) of the ions, each raised to the power represented by its coefficient in the dissociation
equation, is a constant. This special equilibrium constant is called the solubility product constant,
Ksp of that substance. The Ksp of a saturated lead chloride solution can be expressed as:
Ksp = [Pb2+] [Cl-]2
Note:
Cl- concentration is raised to the power of 2, which is the coefficient of this ion in the equilibrium
equation for a saturated solution of PbCl2.
The solubility product constant of a substance must apply at a specific temperature because
solubilities vary with the temperature. Generally, temperature used is 25 °C (298 K).
APPARATUS
Erlenmeyer flask 250 mL, graduated cylinder 10 mL and 100 mL, thermometer, rubber stopper
REAGENTS
0.10 M Pb(NO3)2, 0.020 M KI, distilled water, sodium bicarbonate
PROCEDURE
1. Using appropriate measuring cylinder, measured 5 mL 0.010 M Pb(NO 3)2 and add it to
Erlenmeyer flask. Then, measured exactly 90 mL of distilled water and add it to the flask, swirl
the flask to mix the contents.
2. Using appropriate measuring cylinder, measured 5 mL 0.020 M KI and add it to the mixture in
the flask. Stopper the flask and shake it vigorously to mix the contents thoroughly.
3. Remove the stopper and measure the temperature of the solution. Assume that this
temperature will be the same for all the trials.
4. Allow the flask stand for 7-10 minutes, then check the solution for a cloudy appearance. Record
your observation as Trial 1. Use one of the following to describe the sample:
(a) clear, (b) contains sparkling flakes, (c) shows yellow precipitate.
5. Repeat step 1 through 4 using the volume indicated below:
6. Dispose the solutions and mixtures in the inorganic waste container provided.
Filter all the sample. Then, a hot saturated solution of bicarbonate added to the waste solution
of lead iodide. This caused the solution to go cloudy with a lead carbonate precipitate. The iodide
is still marginally soluble, but the carbonate is truly insoluble. The carbonate precipitate can be
filtered off and disposed of as regular garbage. The solution now contains only potassium nitrate
and baking soda, and can be poured down the drain with plenty of water.
DATA
Temperature = °C
Trial Appearance
1
2
3
4
5
CALCULATIONS
1. Find the number of moles of Pb2+ in the volume of 0.010 M Pb(NO3)2, in which sparkling
flakes first appeared.
2. For every trial, the total volume of the solution of Pb(NO3)2, H2O and KI was 100 mL. Thus,
the number of moles of Pb2+ from calculation 1 was used to make a solution with a volume
100 mL. What was the concentration of the Pb2+ ion in this solution, expressed as molarity?
3. Find the number of moles of I- in the volume of 0.020 M KI in which sparkling flakes first
appeared.
4. The number of moles of I- from calculation 3 was used to make a solution with a volume 100
mL. What was the concentration of the I- ion in this solution, expressed as molarity?
5. Write the solubility product expression for the equilibrium.
6. Calculate the solubility product constant for PbI2 based on the solubility product expression
(calculation 5) and the molar concentrations of Pb2+ (calculation 2) and I- (calculation 4).
DISCUSSION
1. What is the accepted values for the Ksp of PbI2 (refer Table)? How does this value compare
with your experimental result? Discuss.
2. In general, when will a sparingly soluble salt precipitate from solution?
3. Why must some solid remain in contact with a solution of a sparingly soluble salt in order to
ensure equilibrium?
QUESTIONS
1. Write the expression and accepted value for the Ksp of the following salts at 25 °C:
a) ZnCO3
b) BaCrO4
c) Mg(OH)2
d) Ca(IO3)2
2. Calculate the concentration in moles per liters of Ag+ in a saturated solution of the AgCl salt,
using the accepted value for the Ksp at 25 °C in Table.
EXPERIMENT 4
OBJECTIVE
Upon completion the experiment, students should be able to:
1. Determine the solubility product of borax as a function of temperature.
2. Determine the standard free energy, standard enthalpy and standard entropy changes
for the aqueous dissolution of borax.
INTRODUCTION
The relationship between free energy (∆G), enthalpy (∆H), entropy (∆S) and equilibrium constant (K)
for a chemical reaction at a specific temperature (T) is shown in equation (1) below. The gas
constant, R, is equal to 8.314 J/mol.K
∆G° = -R T ln K = ∆H° - T∆S°
Looking at this equation we see that if the reaction is thermodynamically favored, ∆G° < 0, and we
would expect K to be large, K >> 1. If K is much greater than one, we will observe the reaction
proceeding primarily to products.
Rearranging the equation above to eliminate ∆G°, ln K is expressed in terms of ∆H, ∆S and T only:
(−∆𝐾°) 1 (∆𝐾°)
ln 𝐾 = +
( 𝐾 )𝐾 (𝐾)
As long as we can determine the equilibrium constant at several temperatures, this equation is well-
suited for determining ∆H and ∆S by linear regression.
(−∆𝐾°) 1 (∆𝐾°)
ln 𝐾 = +
( 𝐾 )𝐾 (𝐾)
𝐾 = 𝐾.𝐾 + 𝐾
The above expression is valid only if H and S are not temperature dependent quantities. Over the
small temperature range that we shall investigate, this assumption is valid for borax.
Sodium tetraborate dissociates in water to form sodium and borate ions:
Na2[B4O5(OH)4].8H2O(s) 2Na+(aq) + B4O5(OH) 4 2- (aq) + 8H2O
(l)
Note that two sodium ions are produced for each borate ion in the reaction. Therefore, the
concentration of Na+ is TWICE on the concentration of borate ion. If we let ‘s’ represent the
concentration of tetraborate ions in solution at equilibrium, then Na+ ions must equal ‘2s’. Substituting
these values into the equilibrium expression the equation becomes:
Ksp = (2s)2 (s) = 4(s)3
The amount of B4O5(OH)42- in solution is determined by titration with HCl using methyl red as an
indicator. The balanced equation for the titration is:
B4O5(OH) 42- (aq) + 2H+ (aq) + 3H2O 4B(OH)3 (aq)
APPARATUS
Erlenmeyer flask 250 mL, pipette 5 mL, thermometer, burette, beaker 100 mL, measuring cylinder
50 mL, hot plate
REAGENTS
Borax, hydrochloric acid 0.2 M, distilled water, methyl red
PROCEDURE
Temperature (K)
1/T (K-1)
Final burette
reading (mL)
Initial burette
reading (mL)
Volume HCl (mL)
Moles H+
Moles
2-
B4O5(OH)4
Molarity
2-
B4O5(OH)4
Ksp
ln Ksp
CALCULATIONS
1. Plot the natural logarithm of the solubility product (ln Ksp) versus the reciprocal Kelvin
temperature (1/T (K-1) ) for each sample using the EXCEL software.
The data points in the plot can be fit to a straight line by right clicking on a data point and
selecting “Add Trendline” from the menu box. In the fit menu you must select Add Equation
to Chart from the Options tab.
QUESTIONS
1. Based on the values of enthalpy and entropy that you determined for the dissolution of Borax,
what would be the solubility of borax at 85 °C?
2. Name the other indicator could replace the methyl red in this experiment? Give the colour
changes.
OBJECTIVE
Anode Zn Zn Zn
Cathode Cu Fe Pb
Oxidising agent Cu Fe Pb
Reducing agent Zn Zn Zn
Half-reaction for Zn Zn2+ + 2e- Zn Zn2+ + 2e- Zn Zn2+ + 2e-
oxidation
Metal X is Ferum .
Metal Y is Plumbum .
B) Nernst Equation for varying Cu2+ concentration
Explain how you identified unknowns X and Y. Discuss any uncertainty in your identifications.
Discuss about the effect of varying concentration of CuSO4 with the Ecell value of voltaic cell.
In this experiment, we will determine the potential energy of each of full cell, and arrange
it according to the half-reaction of Standard Reduction Potential. As we going down the half-
reaction reduction table, the value of E◦cell will decreasing, but increasing the strength as
reducing agent. Next, if we varying the concentration of CuSO4 with the Ecell value of the
voltaic, this will affect the cell potential value proportionally.
In addition, Electrochemical cell typically consist of two-half cells. The half-cells separate
the oxidation half-reaction from the reduction half-reaction and make it possible for current to
flow trough an external wire. One half-cell, normally depicted on the left side in a figure
contain the anode. Oxidation occur at the anode. The anode is connected to the cathode in
the other half-cell. Reduction occurs at the cathode. Adding a salt bridge completes the
circuit allowing current to flow toward the anode and cations in the salt bridge flow toward
cathode. The movement of these ions completes the circuit. Electrochemical cells can be
described using cell notation. In this notation, the reaction at the anode appears on the left
and information about the reaction at the cathode on the right. Electrodes that do not
participate in the oxidation-reduction reaction but are there to allow current to flow are inert
electrodes. Inert electrodes are often made from platinum or goldm which are unchanged by
many chemical reactions.
QUESTIONS
1. A voltaic cell is constructed coupling a Cu/Cu2+ half-cell with an Ag/Ag+ half-cell. The
concentrations of Cu2+ and Ag+ are each 0.010 M.
a) Which metal is the anode? How do you know?
Anode is Cu metal. This is because in Stamdard Reduction Potentials Table, Cu metal is
lower than the Ag metal. This show that the Cu metal has higher strength as reducing
agent so it will undergo oxidation reaction.
b) Write the half-reaction for the reduction reaction and oxidation reaction.
Reduction reaction: Ag+ (aq) +2e- Ag (s)
Oxidation reaction: Cu (s) Cu2+ (aq) +2e-
c) If the observed potential of the cell, Ecell, is 0.40 V, use the Nernst equation to calculate
the standard cell potential, E°cell.
Cu (s) + 2Ag+ (aq) 2Ag(s) + Cu2+ (aq)
Keq = [ Cu2+]
[Ag+]2
= (0.010M)
(0.010M)2
= 100M
0
E cell= 0.40v- 0.0257ln(100M)
2
= 0.34V
CONCLUSION:
As a conclusion from the experiment, we had develop our understanding of the movement of electrons
and explain the concept of electron flow which are anion and cations. Besides, we also able to
determine the relative potential of reduction for the redox reactions which in this experiment is the
between Zn and Cu which is 0.90V. Moreover, we are able to describe the effect of concentration to
the cell potential.
REFERENCES:
1. https://opentextbc.ca/chemistry/chapter/17-2-galvanic-cells/
2. https://www.thoughtco.com/types-of-electrochemical-cells-606455
3. https://www.corrosionpedia.com/definition/567/galvanic-cell